EP1003038B1 - Appareil de dosage immunologique - Google Patents

Appareil de dosage immunologique Download PDF

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Publication number
EP1003038B1
EP1003038B1 EP98933942A EP98933942A EP1003038B1 EP 1003038 B1 EP1003038 B1 EP 1003038B1 EP 98933942 A EP98933942 A EP 98933942A EP 98933942 A EP98933942 A EP 98933942A EP 1003038 B1 EP1003038 B1 EP 1003038B1
Authority
EP
European Patent Office
Prior art keywords
region
chromatography strip
protective laminate
substrate
partial region
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP98933942A
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German (de)
English (en)
Other versions
EP1003038A4 (fr
EP1003038A1 (fr
Inventor
Miho-Dainabot Co. Ltd. NAKAYA
Ryotaro-Dainabot Co. Ltd. CHIBA
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Abbott Japan Co Ltd
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Abbott Japan Co Ltd
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Filing date
Publication date
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Publication of EP1003038A1 publication Critical patent/EP1003038A1/fr
Publication of EP1003038A4 publication Critical patent/EP1003038A4/fr
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Publication of EP1003038B1 publication Critical patent/EP1003038B1/fr
Anticipated expiration legal-status Critical
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/558—Immunoassay; Biospecific binding assay; Materials therefor using diffusion or migration of antigen or antibody
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
    • G01N33/54366—Apparatus specially adapted for solid-phase testing
    • G01N33/54386—Analytical elements
    • G01N33/54387—Immunochromatographic test strips
    • G01N33/54388—Immunochromatographic test strips based on lateral flow
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/805—Test papers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/81—Packaged device or kit
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/97—Test strip or test slide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S436/00—Chemistry: analytical and immunological testing
    • Y10S436/805—Optical property
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S436/00—Chemistry: analytical and immunological testing
    • Y10S436/807—Apparatus included in process claim, e.g. physical support structures
    • Y10S436/81—Tube, bottle, or dipstick

Definitions

  • This invention relates to an immunoassay device in which a chromatography strip is used. More particularly, it relates to an immunoassay device which consists of a chromatography strip having a substrate adhered to the under surface thereof and a one-piece protective laminate adhered to the top surface thereof, wherein a space is arranged on the top and/or under surface of at least a partial region of a colouring region of said chromatography strip by preventing said partial region from adhering to an area of at least one of surfaces of the protective laminate and substrate which area faces on said partial region.
  • a system is arranged so that an added sample solution to be tested can move in the chromatography strip by the force of capillary flow, and a detecting region of an analyte is arranged on a downstream part of a region where the sample solution is added.
  • the detecting region is arranged in such a manner that it develops a colour or its colouring degree is reduced when a sample solution arrived thereto contains an analyte, so that the presence or quantity of the analyte can be detected or measured based on the colouring degree of the detecting region.
  • JP-A-61-145459 the term “JP-A” as used herein means an "unexamined published Japanese patent application”
  • JP-A-64-32169 JP-A-1-113662
  • JP-A-244370 JP-A-1-63865
  • JP-W-1-503174 the term “JP-W” as used herein means an "unexamined published Japanese international patent application”
  • Each of these immunoassay devices has a chromatography strip in which a substrate is adhered to the under surface thereof and a protective laminate is adhered to the top surface thereof, in order to protect the chromatography strip and prevent biohazard.
  • the capillary flow of sample solution is not uniform in a region of a chromatography strip where analytical reagents are immobilized such as a coloring region.
  • a coloring region When the flow of a sample solution is not uniform in a coloring region, development of color in the coloring region becomes so irregular that white spots and the like are formed in the coloring region, thus causing reduction of the detection accuracy.
  • WO 94/15215 discloses a test strip for rapid immunoassays, containing Specific immunochemical reagent zones.
  • WO 96/33413 discloses a lateral flow immunochromatographic assay device without a plastic housing.
  • WO 93/24231 discloses diagnostic devices and apparatus for the controlled movement of reagents without membranes.
  • EP-A-0 420 021 discloses hydrophillic laminated porous membranes and methods of preparing same.
  • WO 92/08972 discloses an improved agglutination reaction device having geometrically modified chambers.
  • the object of the present invention is to provide an immunoassay device in which a chromatography strip is used in such a manner that capillary flow of a sample solution in its colouring region becomes uniform.
  • the inventors of the present invention have found that white spots and the like problems caused by irregular capillary flow in a colouring region do not occur and high detection accuracy can be obtained when a space is arranged in at least a partial region of the colouring region in a chromatography strip which has a substrate adhered to the surface thereof and a protecting laminate adhered to the top surface thereof.
  • a similar solution has been disclosed in EP 0 821 235-A, which is prior art under Article 54(3) and (4) EPC. However, this document does not relate to chromatography strips having a colouring region downstream of a sample applying region.
  • the present invention is an immunoassay device which consists of a chromatography strip having a substrate adhered to the under surface thereof and a one-piece protective laminate adhered to the top surface thereof, wherein a space is arranged on the top and/or under surface of at least a partial region of a colouring region of said chromatography strip by having a means for preventing said partial region from adhering to an area of at least one of surfaces of the protective laminate and substrate which area faces on said partial region, wherein the colouring region is at a position downstream of a sample applying region.
  • the immunoassay device of the present invention has a chromatography strip (1) in which a substrate (2) is adhered to its under surface and a protective laminate (3) is adhered to its top surface.
  • chromatography carrier of the chromatography strip any of those which are known in this field can be used.
  • cellulose, nitrocellulose, cellulose acetate and the like are used most frequently.
  • the substrate and protective laminate are adhered to the chromatography strip by applying a paste (4) to the substrate and protective laminate.
  • a paste (4) for example, a rubber, acrylic, vinyl ether polymer or the like adhesive is used as the paste.
  • the chromatography carrier and the substrate may be adhered by dissolving nitrocellulose in an organic solvent such as acetone or the like and spreading the solution on a substrate composed of polyethylene terephthalate or the like film which is soluble in the solvent or on a substrate having the same film. Such a case is also included in the adhering of the chromatography strip to the substrate of the present invention.
  • the substrate and protective laminate may be those which are usually used in the conventional immunoassay devices in which chromatography strips are employed.
  • polyethylene terephthalate, polypropylene, polyvinyl chloride and the like may be used.
  • the chromatography strip has a sample applying region (5), and when a sample solution having a possibility of containing an analyte is applied to the sample applying region, the sample solution moves to the downstream direction by the force of capillary flow.
  • the chromatography strip also has a coloring region at a downstream position of the sample applying region.
  • the coloring region is a region which develops color during the assay, and it includes a detecting region (6) for detecting an analyte in a sample solution.
  • a control region (7) may be arranged as a coloring region.
  • the detecting region is arranged in such a manner that a tracer comprised of a labeled antigen or antibody is accumulated in response to the presence or quantity of an analyte contained in a sample solution which is migrated form the upstream area by the force of capillary flow.
  • a tracer comprised of a labeled antigen or antibody is accumulated in response to the presence or quantity of an analyte contained in a sample solution which is migrated form the upstream area by the force of capillary flow.
  • the term "in response to the presence or quantity of an analyte” as used herein means that the amount of accumulated tracer increases in the case of a sandwich assay or the amount of accumulated tracer decreases in the case of a competitive assay.
  • the detecting region contains an immobilized compound to which, if necessary via a certain crosslinking compound, an analyte specifically binds (in this case, a tracer binds specifically to the analyte also) or specifically binds in competition with the tracer.
  • crosslinking compound means a substance which binds specifically to both of the compound immobilized to the detecting region and an analyte.
  • an anti-mouse IgG antibody is immobilized to the detecting region and a mouse IgG for an analyte antigen is used as the crosslinking compound.
  • the crosslinking compound a conjugate composed of a compound which specifically binds to the compound immobilized to the detecting region and a substance that specifically binds to an analyte.
  • the substance that specifically binds to an analyte may be an antibody when the analyte is an antigen, or an antigen when the analyte is an antibody.
  • the combination of a compound immobilized to the detecting region and a compound which specifically binds to the compound immobilized to the detecting region may be biotin as one and anti-biotin antibody or avidin as the other, or a saccharide as one and a saccharide-binding protein as the other.
  • a second detecting region may be arranged at a position downstream of the detecting region, in order to capture the tracer which has not been captured at the detecting region. This second detecting region is also included in the "detecting region" of the present invention.
  • Examples of the marker to be used include enzymes relating to coloring developing reactions, gold colloid and the like metal colloids, selenium colloid and the like non-metal colloids, and colored resin microparticles, colored liposomes, dyestuff microparticles and the like colored microparticles.
  • coloring degree of the detecting region changes when the tracer is accumulated or not accumulated in the detecting region, whereby the presence or quantity of an analyte in a sample solution can be known by measuring the coloring degree with the naked eye or using an instrument.
  • the control region is a region which is employed to know if a sample solution has properly passed through the detecting region, and is arranged, when required, in such a manner that the control region develops a color when the sample solution reaches the control region.
  • the control region is arranged at a position downstream of the detecting region as occasion demands. Development of color when a sample solution reaches the control region can be effected by a well known method, for example by including a pH indicator, an enzyme which takes charge of the coloring reaction or a tracer in the sample solution and immobilizing a compound to the control region which develops a color when such a substance reaches the region.
  • the tracer may be included in advance in a specified region (labeling region (8)) of the chromatography strip or added together with a sample solution when the sample solution is applied.
  • top surface as used herein means the side of chromatography strip which the protective laminate is adhered to
  • under surface means the side of chromatography strip which the substrate is adhered to.
  • space means a part where the protective laminate or substrate is not adhered to the chromatography strip surface.
  • capillary flow of a sample solution is not disturbed when a space is arranged only in a partial region of the coloring region, so the space can be arranged at least a partial region of the coloring region.
  • the space does not exert its effect when the partial region of the coloring region is extremely small as a matter of course, and further it becomes difficult not to paste the partial region when the partial region of the coloring region is too small.
  • the upstream and downstream regions may have any extent, provided that they are not the entire portion of the chromatography strip.
  • the space may be arranged either on the under or top surface of the chromatography strip or on both of the top and under surfaces.
  • Arrangement of the space can be effected by not pasting together at least a partial region of the coloring region and the surface of the protective laminate and/or substrate which faces on said region (Fig. 1 and Fig. 2). Not to paste a partial region of the coloring region and the protective laminate and/or substrate together, a paste is not applied to the non-pasting part of the protective laminate, or, when the paste is applied, an agent capable of invalidating adhesive property of the paste is applied to the non-pasting part. All of known agents can be used as the agent capable of invalidating adhesive property of the paste.
  • the adhering preventing method may be the same or different from one another.
  • a method in which both of the protective laminate and substrate are not covered is not desirable, because it will cause damages such as bending of the chromatography strip.
  • a nitrocellulose film (manufactured by Millipore, U.S.A.) of 0.5 cm x 4.0 cm in size was stuck on a substrate ("Pack Laminate").
  • a solution containing a syphilis antigen derived from Treponema pallidum was spotted in a line on a position about 1 cm from its bottom end and thoroughly dried to immobilize the syphilis antigen, thereby arranging a detecting region on the nitrocellulose film.
  • avidin was immobilized on the nitrocellulose film about 1 cm upside from the detecting region, thereby arranging a control region.
  • a glass fiber film (manufactured by Lydall, U.S.A.) was impregnated with a labeled antigen obtained by labeling the syphilis antigen derived from Treponema pallidum with selenium colloid and with biotinated selenium colloid obtained by binding biotin to selenium colloid, and then the glass fiber film was dried to be used as a labeling region.
  • the thus prepared labeling region was stuck on the substrate in such a manner that it slightly contacted with the bottom end of the previously obtained nitrocellulose film on the substrate.
  • a non-woven fabric manufactured by Du Pont, U.S.A.
  • 0.5 x 1.0 cm in size was stuck on the substrate at the bottom end of the labeling region so that it contacted with the labeling region.
  • a protective laminate (manufactured by Lintech) is stuck on the top surface of the chromatography strip obtained in the above manner, and detection of syphilis antibody in a sample to be tested is carried out using the thus obtained chromatography strip device.
  • a 50 ⁇ l portion of a serum sample to be tested is applied to the sample applying region of the chromatography strip device, and the result is judged 15 minutes after application of the serum by reading with the naked eye "redness" of the selenium colloid in the detecting region and control region.

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  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Molecular Biology (AREA)
  • Biomedical Technology (AREA)
  • Chemical & Material Sciences (AREA)
  • Hematology (AREA)
  • Urology & Nephrology (AREA)
  • Biotechnology (AREA)
  • Biochemistry (AREA)
  • Cell Biology (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Microbiology (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

L'invention concerne un appareil de dosage immunologique comportant une bande chromatographique présentant un substrat collé sur sa surface inférieure et un stratifié de protection collé sur sa surface supérieure, un espace étant situé sur la surface supérieure et/ou inférieure d'au moins une partie d'une zone de développement de couleur de la bande chromatographique. Dans l'appareil selon l'invention, des flux capillaires d'un échantillon liquide dans la zone de développement de couleur de la bande chromatographique sont homogènes, ce qui permet d'obtenir une haute précision de détection.

Claims (3)

  1. Dispositif de dosage immunologique qui se compose d'une bandelette de chromatographie (1) comprenant un substrat (2) collé à la surface inférieure de celle-ci et un stratifié protecteur d'une seule pièce (3) collé à la surface supérieure de celle-ci, dans lequel un espace (9) est formé sur la surface supérieure et/ou inférieure d'au moins une région partielle d'une région colorante de ladite bandelette de chromatographie en ayant un moyen pour empêcher que ladite région partielle n'adhère à une zone d'au moins une des surfaces du stratifié protecteur et du substrat, laquelle zone fait face à ladite région partielle, dans lequel la région colorante se trouve à une position en aval d'une région d'application d'échantillon (5).
  2. Dispositif de dosage immunologique selon la revendication 1, dans lequel ledit moyen pour empêcher que ladite région partielle n'adhère à ladite zone d'au moins une desdites surfaces du stratifié protecteur et du substrat, laquelle zone fait face à ladite région partielle, est formé en n'appliquant pas de colle sur ladite zone d'au moins une desdites surfaces.
  3. Dispositif de dosage immunologique selon la revendication 1, dans lequel ledit moyen pour empêcher que ladite région partielle n'adhère à ladite zone d'au moins une desdites surfaces du stratifié protecteur et du substrat, laquelle zone fait face à ladite région partielle, est formé en appliquant un agent capable d'invalider la propriété adhésive d'une colle sur ladite zone d'au moins une desdites surfaces.
EP98933942A 1997-07-28 1998-07-27 Appareil de dosage immunologique Expired - Lifetime EP1003038B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP20188897 1997-07-28
JP20188897A JP3655990B2 (ja) 1997-07-28 1997-07-28 免疫分析装置
PCT/JP1998/003334 WO1999005526A1 (fr) 1997-07-28 1998-07-27 Appareil de dosage immunologique

Publications (3)

Publication Number Publication Date
EP1003038A1 EP1003038A1 (fr) 2000-05-24
EP1003038A4 EP1003038A4 (fr) 2002-09-04
EP1003038B1 true EP1003038B1 (fr) 2007-02-14

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Application Number Title Priority Date Filing Date
EP98933942A Expired - Lifetime EP1003038B1 (fr) 1997-07-28 1998-07-27 Appareil de dosage immunologique

Country Status (11)

Country Link
US (2) US6537828B1 (fr)
EP (1) EP1003038B1 (fr)
JP (1) JP3655990B2 (fr)
KR (1) KR20010012406A (fr)
CN (1) CN1158525C (fr)
AU (1) AU8358398A (fr)
CA (1) CA2289713C (fr)
DE (1) DE69837092T2 (fr)
HK (1) HK1025385A1 (fr)
WO (1) WO1999005526A1 (fr)
ZA (1) ZA986678B (fr)

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JP4402263B2 (ja) * 1999-06-21 2010-01-20 パナソニック株式会社 クロマトグラフィー定量測定装置
KR100485564B1 (ko) * 2000-04-28 2005-04-28 마츠시타 덴끼 산교 가부시키가이샤 크로마토그래피 측정 장치
US7575915B2 (en) 2000-05-26 2009-08-18 Panasonic Corporation Biosensor
KR100497020B1 (ko) * 2000-05-29 2005-06-23 마츠시타 덴끼 산교 가부시키가이샤 바이오센서 및 그의 제조 방법
US6783992B2 (en) * 2001-01-03 2004-08-31 Agilent Technologies, Inc. Methods and using chemico-mechanical microvalve devices for the selective separation of components from multi-component fluid samples
ATE550657T1 (de) 2001-04-12 2012-04-15 Arkray Inc Probenanalysegerät
KR100455298B1 (ko) * 2001-06-15 2004-11-09 주)녹십자 투명한 플라스틱 지지체를 가진 면역크로마토그래피 분석 디바이스 및 그의 제조 방법
US20040219691A1 (en) * 2003-04-29 2004-11-04 Shartle Robert J. Test strip with clear base support layer for visual perception of a liquid sample during application
US20070207496A1 (en) * 2004-11-19 2007-09-06 Larsen Oeistein Diagnostic control system
JP4773909B2 (ja) * 2005-09-27 2011-09-14 シスメックス株式会社 イムノクロマトグラフィー用キット、試験容器
US7344893B2 (en) * 2005-10-13 2008-03-18 Auric Enterprises, Llc Immuno-gold lateral flow assay
US8153444B2 (en) * 2005-10-13 2012-04-10 Auric Enterprises, Llc Immuno gold lateral flow assay
US8956859B1 (en) 2010-08-13 2015-02-17 Aviex Technologies Llc Compositions and methods for determining successful immunization by one or more vaccines
ES2645468T3 (es) 2012-07-06 2017-12-05 Ngk Insulators, Ltd. Herramienta de inspección para cromatografía de ácidos nucleicos
KR102065001B1 (ko) * 2016-10-12 2020-01-10 한국전자통신연구원 투광성 면역 검사 장치 및 방법

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Also Published As

Publication number Publication date
EP1003038A4 (fr) 2002-09-04
EP1003038A1 (fr) 2000-05-24
WO1999005526A1 (fr) 1999-02-04
HK1025385A1 (en) 2000-11-10
US6537828B1 (en) 2003-03-25
CN1158525C (zh) 2004-07-21
JPH1144689A (ja) 1999-02-16
CN1257581A (zh) 2000-06-21
DE69837092D1 (en) 2007-03-29
DE69837092T2 (de) 2007-12-06
US20020094585A1 (en) 2002-07-18
JP3655990B2 (ja) 2005-06-02
ZA986678B (en) 1999-02-04
AU8358398A (en) 1999-02-16
CA2289713C (fr) 2008-03-11
CA2289713A1 (fr) 1999-02-04
KR20010012406A (ko) 2001-02-15

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